Hydrochloric Acid → HCID 178473964、化合物

HRID 1637954

反応式

HRID 1637954 の反応式
[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([N+:13]([O-:15])=[O:14])=[CH:10][CH:11]=2)[CH2:6][C:5]1=[O:16])(=[O:3])[CH3:2].[F:17][C:18]([F:29])([F:28])[C:19]1[CH:27]=[CH:26][C:22]([C:23](O)=[O:24])=[CH:21][CH:20]=1.CN(C(ON1N=NC2C=CC=CC1=2)=[N+](C)C)C.[B-](F)(F)(F)F.C1C=CC2N(O)N=NC=2C=1.Cl>CN(C=O)C>[C:1]([N:4]1[C:12]2[C:7](=[CH:8][C:9]([N+:13]([O-:15])=[O:14])=[CH:10][CH:11]=2)[C:6](=[C:23]([OH:24])[C:22]2[CH:26]=[CH:27][C:19]([C:18]([F:17])([F:28])[F:29])=[CH:20][CH:21]=2)[C:5]1=[O:16])(=[O:3])[CH3:2]

参加物

7

反応物 5

HCID 313Hydrochloric AcidHCID 99664-(Trifluoromethyl)benzoic acidHCID 757711-HydroxybenzotriazoleHCID 2733207O-(Benzotriazol-1-yl)-N,N,N',N'-tetramethyluronium tetrafluoroborateHCID 28393291-Acetyl-5-nitroindolin-2-one

生成物 1

HCID 178473964HCID 178473964、化合物

試薬・触媒・溶媒 1

HCID 6228Dimethylformamide溶媒

実験手順

Prepared by reacting 1-acetyl-5-nitro-2-indolinone with one equivalent of 4-trifluoromethyl-benzoic acid in dry DMF in the presence of 1 equivalent each of TBTU and HOBT and 5 equivalents of Huinig's base (20° C., 4 hours), stirring into dilute hydrochloric acid, filtering the precipitate, dissolving the precipitate in EtOac, drying the organic phase and evaporation in vacuo and purifying the evaporation residue by column chromatography on silica gel with CH2Cl2 /MeOH (10:1) as eluant.

後処理

  1. customPrepared
  2. filtrationfiltering the precipitate
  3. dissolutiondissolving the precipitate in EtOac
  4. customdrying
  5. customthe organic phase and evaporation in vacuo
  6. custompurifying the evaporation residue by column chromatography on silica gel with CH2Cl2 /MeOH (10:1) as eluant

出典と根拠

ORDレコード
ord-ced276462a764a7a8b4fce8abba231b5
出典データセット
uspto-grants-2000_03
特許番号
US06043254

関連ノート

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